CN103646868A - Method for preparing porous silicon by adopting hydrothermal-vapor etching - Google Patents

Method for preparing porous silicon by adopting hydrothermal-vapor etching Download PDF

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CN103646868A
CN103646868A CN201310544260.0A CN201310544260A CN103646868A CN 103646868 A CN103646868 A CN 103646868A CN 201310544260 A CN201310544260 A CN 201310544260A CN 103646868 A CN103646868 A CN 103646868A
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silicon
porous silicon
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vapor
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CN103646868B (en
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石明吉
张戈
郭新峰
丁淑娟
张又华
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Nanyang Institute of Technology
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    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02002—Preparing wafers
    • H01L21/02005—Preparing bulk and homogeneous wafers
    • H01L21/0203—Making porous regions on the surface
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    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02002—Preparing wafers
    • H01L21/02005—Preparing bulk and homogeneous wafers
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Abstract

The invention relates to a method for preparing porous silicon by adopting hydrothermal-vapor etching. The method comprises the steps of processing a silicon substrate, heating a reaction liquid by a hydrothermal reaction kettle, arranging a monocrystalline silicon piece bracket above the reaction liquid, placing the reaction kettle in an oven with a temperature of 130 DEG C-190 DEG C to react, enabling the reaction liquid to generate acid vapor, and etching the silicon piece above the reaction liquid so as to obtain the porous silicon. The porous silicon capable of emitting red light stably can be acquired through regulating the reaction temperature and the reaction time. The method provided by the invention is good in repeatability, and a prepared porous silicon sample has the advantages of large light-emitting area, stable light emission, high light-emitting intensity, smooth surface and the like.

Description

Hydro-thermal-vapor etch legal system is for the method for porous silicon
Technical field
The invention belongs to semiconductor silicon material preparing technical field, be specifically related to a kind of simple, fast and efficient porous silicon preparation method.
Technical background
Along with the development of information technology, people have proposed high request more to the transmission speed of information, storage capacity, processing capacity.Semi-conducting material particularly silicon-chip technology and photoelectron material and device technology is the basis of information technology, and the integrated circuit growing up on silicon materials becomes development electronic computer, communication and the key of the information technologies such as control automatically.In order to realize integrated-optic device and luminescent device on same silicon chip, namely photoelectron is integrated, and development silicon base luminous material and device become the vital task that 21 century scientist need to solve.
Nineteen ninety, Canham further corrodes after a few hours by porous silicon in HF solution, with blue light or UV-irradiation porous silica material, in room temperature, observe very strong ruddiness, this discovery makes the luminescence studies of relevant porous silicon enter a new stage, thereby has shown microelectronics and photoelectron are integrated in to the possibility on same silicon chip.1996, the people such as Hirschman integrated porous silicon luminescence pipe and silicon planar transistor, had made a photoelectron integrated light-emitting array, and this is the integrated the first of porous silicon photoelectron, is an important breakthrough, shows the feasibility that porous silicon photoelectron is integrated.
Existing research shows, the micro-structural of porous and luminosity thereof depend on its preparation technology and condition.At present, the method for preparing porous silicon mainly contains electrochemical erosion method, stain etch, photochemical corrosion method, spark-discharge method, pulsed etching method, etching method, hydrothermal etching etc.
In electrochemical erosion method, adopt platinum filament to make negative electrode, monocrystalline silicon piece is made anode and in HF solution, is carried out electrochemical corrosion, relative position insulation effect improper and bubble hydrogen that silicon chip surface forms between anode and negative electrode all can cause the spatial variations of current density, thereby causes the generation of non-uniform corrosion.Its direct result is: cause silicon silk size to there is wider distribution, and unfavorable to exploring luminous mechanism; Porous rete is frangible, and the intensity of monoblock sample is low, is difficult to use in the making of device.On the other hand, the resulting porous silicon surface of electrochemical erosion method is the interference color of khaki or inhomogeneous form, does not have the smooth finish surface of polishing monocrystalline silicon, also to application, is provided with obstacle.
Stain etch method claims again corrosion, by preparing suitable corrosive liquid, directly monocrystalline silicon piece is carried out to chemical corrosion and prepares porous silicon.Advantage is without bias voltage, and preparation technology is simple, if grow porous silicon in dielectric substrate, this method is more useful; Shortcoming is that the luminous efficiency of goods is lower, and the uniformity of material structure is poor, and experiment repetition rate is low.In addition, the method exists equally because bubble hydrogen causes the problem of non-uniform corrosion in adhering to of silicon chip surface.
Photochemical corrosion method is under the effect of light, and the crystalline silicon being immersed in the HF aqueous solution or ethanolic solution reacts with HF.Illumination can produce non equilibrium carrier in crystalline silicon, and the necessary electronics of reaction and hole are provided, and accelerates surperficial reaction speed.In the method, if incident light wavelength is oversize, the energy of photon can be less than the energy gap of silicon and can not produce electron-hole pair; If incident light wavelength is too short, can compared with large absorption, affect the output capacity of electron-hole pair because of silicon chip surface again.
Etching method is divided into three kinds of ise, vapor etch and gas etching methods.Ise is that the solution containing HF acid is passed through to nozzle, with certain speed, be ejected into bulk silicon substrate surface, and then grow porous silicon, but because the higher HF drop of relative speed is when clashing into silicon substrate, can be launched other regions, can be affected the quality of figure.Vapor etch method is silicon chip to be exposed to the HNO of finite concentration ratio 3in the steam of HF mixture.Silicon substrate is placed in the top of acid etch groove, by heating etching liquid, produces steam, and then forms porous silicon.With the porous silicon that this method forms, have the features such as inexpensive, layer is thin and even, be highly suitable in solar energy in large area battery and do antireflective coating use, its reflectivity is no more than 4%.At present, the method only limits to the preparation of large area porous silicon layer, and application in other respects need further exploitation.Gas etching method is respectively by heating NO 2, O 2with HF acid solution, obtain the mist that temperature is higher, monocrystalline silicon piece is positioned under the environment of this mist and carries out etching, make porous silicon.
Hydrothermal etching is seminar of China Chinese University of Science and Technology proposes hydro-thermal corrosion a kind of new porous silicon preparation method for the preparation of porous silicon.Its concrete preparation process is: the monocrystalline silicon piece cutting is first soaked to 15min with acetone or alcohol, to remove the organic pollution of surface attachment, more repeatedly rinse well with distilled water; Silicon chip is fixed in the inner core of high pressure water heating kettle; The corrosive liquid that injection prepares (HF, HF+HNO 3solution etc.), heat treatment 1 ~ 3h at 100 ~ 250 ℃, and naturally cool to room temperature; From water heating kettle, take out sample, with distilled water immersion, clean, then under air at room temperature, naturally dry.By controlling composition, concentration and other preparation condition etc. of corrosive liquid, can obtain the porous silicon of ruddiness, blue light and ultraviolet light emission.The porous silicon of preparing with conventional method is compared, and microstructure is similar, stable luminescence, and luminous intensity is high, and mechanical energy is good, and the preparation repetition rate of sample is high, and without reprocessing.But the problems such as Photoluminescence Intensity of Porous Silicon prepared by hydrothermal etching decay, luminous peak position blue shift not yet solve.In order thoroughly to overcome the above problems, seminar of Chinese University of Science and Technology has proposed again employing original position iron passivation hydrothermal etching and has prepared porous silicon.
Summary of the invention
The object of the invention is to propose a kind ofly can to prepare that light-emitting area is large, stable luminescence, luminous intensity are good, hydro-thermal-vapor etch legal system of any surface finish, reproducible red emission is for the method for porous silicon.
The technical scheme that technical solution problem of the present invention adopts is: a kind of hydro-thermal-vapor etch legal system, for the method for porous silicon, is characterized in that preparing in the steps below:
Figure 2013105442600100002DEST_PATH_IMAGE001
process silicon substrate, use successively acetone and absolute ethyl alcohol ultrasonic cleaning 10min to remove surface and oil contaminant the monocrystalline silicon piece cutting, use again the mixed liquor being mixed by the volume ratio of 3:1 by sulfuric acid and hydrogen peroxide to boil 5min, to remove surface oxide layer, and then use successively acetone and absolute ethyl alcohol ultrasonic cleaning 10min, finally with distilled water flushing, dry standby;
Figure 432302DEST_PATH_IMAGE002
the reactant liquor being mixed by the volume ratio of 23:19:1 by hydrofluoric acid, distilled water and nitric acid is injected into autoclave inside liner, and compactedness is 70% ~ 90%;
Figure 2013105442600100002DEST_PATH_IMAGE003
with support by the monocrystalline silicon horse 2mm ~ 8mm above reactant liquor cleaning;
Figure 640560DEST_PATH_IMAGE004
mounted reactor is put into baking box, and 130 ℃ ~ 190 ℃ temperature ranges, insulation 40 ~ 80min, takes out reactor, with running water, rinses and is down to room temperature;
Figure 2013105442600100002DEST_PATH_IMAGE005
from hydrothermal reaction kettle, take out sample, with distilled water, repeatedly rinse well, then under air at room temperature, naturally dry.
Hydro-thermal-vapor etch method of the present invention and hydro thermal method are completely different, and hydro thermal method is immersed in silicon chip in reactant liquor, and hydro-thermal-vapor etch method by silicon wafer support above reactant liquor liquid level; Hydro-thermal-vapor etch method is also different from traditional vapor etch method, the reaction temperature of traditional vapor etch method is low, generally below 100 ℃, need special equipment, as: thermostat, heater, temperature probe and thermoregulator etc., and the reaction temperature of hydro-thermal-vapor etch method is high, at 130 ℃ ~ 190 ℃, without Special Equipment, only by hydrothermal reaction kettle and conventional oven.
Mechanism of the present invention and technical characterstic:
Silicon wafer support is more than the liquid level of hydrothermal reaction kettle, and the reactant liquor that heating is mixed by hydrofluoric acid, water and nitric acid, makes reactant liquor produce acid vapor, and then silicon chip is produced to corrosion, thereby make porous silicon.Silicon substrate is arranged on the above 2mm ~ 8mm of liquid level, and respond temperature and the silicon chip of the volume ratio of fluid component, reactant liquor of the principal element that affects etching effect is exposed to the time in acid vapor.
At a certain temperature, the acid vapor in the above space of hydrothermal reaction kettle liquid level reaches capacity.Along with the rising of temperature, the critical point that the amount of acid vapor can reach capacity and atomization, this makes hydrothermal reaction kettle inwall and surface of silicon be covered with droplet.The size of drop depends on the roughness of surface of silicon and the saturation of acid vapor.If silicon substrate is too coarse, acid droplet may merge and cause the formation of continuous liquid film.Liquid film can destroy the surface of porous silicon layer or the carrying out that stops hydro-thermal-vapor etch process continuously.
Along with the increase of nitric acid and hydrofluoric acid volume ratio, the content of nitric acid in acid vapor can increase, and the temperature that improves reactant liquor also can make the content of nitric acid in acid vapor strengthen.Guarantee acid vapor stability of flow, must control the temperature of hydrothermal reaction kettle well, according to the dynamic law of etching process, it is very important keeping acid vapor stability of flow.When reacting liquid temperature is low, etching speed is also little; Temperature improves, and etching speed can be accelerated; If reacting liquid temperature is too high, acid droplet may be merged into large drop and destroy rapidly porous silicon layer.The advantage of hydro-thermal-vapor etch method is that method is simple, cost is low, porous silicon layer is thin and even, any surface finish and luminous intensity large.
The conventional method of preparing porous silicon is electrochemical erosion method, but the porous silicon that the method makes corrosion is inhomogeneous, and rete mechanical strength is low and frangible, cannot obtain the much higher hole of luminous intensity silicon, also has luminous unstable, the problem such as luminous efficiency is low simultaneously.The porous silicon that the present invention adopts hydro-thermal-vapor etch method to make not only has bright and clean surface but also has very strong luminescence generated by light, and its luminous intensity is approximately 10 times of the prepared porous silicon of electrochemical erosion method, is 8 times of the prepared porous silicon of vapor etch method.Compared with prior art, hydro-thermal-vapor etch method of the present invention has: simple to operate, cost is low, repetition rate is high, layer is thin, even, be particularly suitable for preparing large-area porous silicon sample.
Accompanying drawing explanation
Fig. 1 is that hydro-thermal-vapor etch method is at HF:H 2o:HNO 3volume ratio be 23:19:1, compactedness is 80%, silicon chip is 3mm to reactant liquor liquid level distance, reaction temperature is 140 ℃, under the condition that the reaction time is 60min, the stereoscan photograph of the porous silicon sample making.
Fig. 2 utilizes the photoluminescence spectrum of porous silicon sample prepared by hydro-thermal-vapor etch method and electrochemical erosion method.
Fig. 3 utilizes the photoluminescence spectrum of hydro-thermal-vapor etch method and the standby porous silicon sample of vapor etch legal system.
Embodiment
Hydro-thermal-vapor etch legal system, for a method for porous silicon, is characterized in that preparing in the steps below:
1, process silicon substrate: by thickness, be that 625um, resistivity are that the P type silicon chip of 8 Ω cm～12 Ω cm, single-sided polishing is used respectively acetone and absolute ethyl alcohol ultrasonic cleaning 10min, remove dust and the greasy dirt of silicon chip surface, and then use the mixed liquor being mixed by the volume ratio of 3:1 by sulfuric acid and hydrogen peroxide to boil 5 min, remove surperficial oxide layer, use respectively again acetone and absolute ethyl alcohol ultrasonic cleaning 10 min, finally with distilled water flushing, dry standby.
2, preparation reaction solution: measure hydrofluoric acid (content>=40%) 10.35ml, nitric acid (content 65%-68%) 0.45ml, distilled water 8.55ml, is mixed with reaction solution 19.5ml ,being poured into cleaned volume is in the reactor inner core of 25ml, and filling rate is 70% ~ 90%, and preferred filling rate is 80%;
3, with the plastic cross support of a resistance to strong acid and 200 ℃ of high temperature, be used for supporting silicon chip, prevent that silicon chip from directly contacting with reactant liquor, above-mentioned support is put into reactor inner core, a top of the trellis exceeds 3mm than reactant liquor liquid level, and silicon chip is lain on support; Wherein silicon chip exceeds 2mm ~ 8mm than reactant liquor liquid level and all can;
4, after reactor sealing, put into baking box, be warming up to 140 ℃, temperature retention time is 60min, after reaction finishes, takes out reactor and rinses and be cooled to room temperature with running water;
5, from hydrothermal reaction kettle, take out sample, with distilled water, repeatedly rinse sample surfaces, remove the corrosive liquid of remained on surface, at room temperature naturally dry.
Porous silicon test result prepared by said method
Utilize scanning electron microscopy (FEI-QUANTA200) to characterize the surface topography of porous silicon.At HF:H 2o:HNO 3volume ratio be 23:19:1, compactedness is 80%, silicon chip is 3mm to reactant liquor liquid level distance, reaction temperature is 140 ℃, and under the condition that the reaction time is 60min, the porous silicon surface making is bright and clean, there is obvious loose structure and bore hole size more consistent, as shown in Figure 1.
The photoluminescence spectrum of the photoluminescence spectrum of the porous silicon sample that hydro-thermal-vapor etch method is prepared under these conditions and porous silicon sample prepared by electrochemical erosion method more as shown in Figure 2.The experiment condition that electrochemical erosion method is prepared porous silicon sample is: take thickness as 625um, resistivity be 8 Ω cm～12 Ω cm, the P type silicon chip (back side copper facing) of single-sided polishing is anode, take platinum filament as negative electrode, the volume ratio of hydrofluoric acid and absolute ethyl alcohol is 1:1.5, temperature is room temperature, electric current is 60mA, and the reaction time is 43min, and platinum filament is 20mm to the distance of silicon chip.
The photoluminescence spectrum of the porous silicon sample that the photoluminescence spectrum of the porous silicon sample that hydro-thermal-vapor etch method is prepared under these conditions and vapor etch legal system are standby more as shown in Figure 3.Vapor etch legal system for the experiment condition of porous silicon sample is: thickness is that 625um, resistivity are 8 Ω cm～12 Ω cm, and the P type silicon chip of single-sided polishing, first uses each ultrasonic cleaning of acetone and absolute ethyl alcohol 10min, uses H 2sO 4: H 2o 2=3:1(volume ratio) mixed liquor boils 5min, with distilled water, cleans and dries.Selecting volume is the polytetrafluoro container of 250ml, configuration HNO 3: HF=1:4(volume ratio) solution 180ml, pours into after polytetrafluoro container, with self-control support, the silicon wafer support of handling well is located to liquid level top 2.5cm, cover lid.Polytetrafluoro container is put in thermostatic drying chamber, at 40 ℃ of reaction 12min.After reaction finishes, take out distilled water flushing for silicon chip, dry.
Result shows, adopts above-mentioned hydro-thermal-vapor etch legal system for porous silicon sample, and surface is very bright and clean, and luminescence generated by light spectral intensity (PL spectral intensity) is 10 times that electrochemical erosion method is prepared sample, is that vapor etch legal system is for 8 times of sample.The method is simple, cost is low, and layer is thin, be applicable to evenly, very much the large-area porous silicon sample of preparation.

Claims (1)

1. hydro-thermal-vapor etch legal system, for a method for porous silicon, is characterized in that preparing in the steps below:
process silicon substrate, use successively acetone and absolute ethyl alcohol ultrasonic cleaning 10min to remove surface and oil contaminant the monocrystalline silicon piece cutting, use again the mixed liquor being mixed by the volume ratio of 3:1 by sulfuric acid and hydrogen peroxide to boil 5min, to remove surface oxide layer, and then use successively acetone and absolute ethyl alcohol ultrasonic cleaning 10min, finally with distilled water flushing, dry standby;
Figure 113882DEST_PATH_IMAGE002
the reactant liquor being mixed by the volume ratio of 23:19:1 by hydrofluoric acid, distilled water and nitric acid is injected into autoclave inside liner, and compactedness is 70% ~ 90%;
Figure 380915DEST_PATH_IMAGE003
with support by the monocrystalline silicon horse 2mm ~ 8mm above reactant liquor cleaning;
Figure 891400DEST_PATH_IMAGE004
mounted reactor is put into baking box, and 130 ℃ ~ 190 ℃ temperature ranges, insulation 40 ~ 80min, takes out reactor, with running water, rinses and is down to room temperature;
Figure 560279DEST_PATH_IMAGE005
from hydrothermal reaction kettle, take out sample, with distilled water, repeatedly rinse well, then under air at room temperature, naturally dry.
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CN105417518A (en) * 2014-09-05 2016-03-23 中国科学院金属研究所 Gas-phase post-treatment modification apparatus and gas-phase post-treatment modification method of solid carbon material
CN105633422A (en) * 2016-03-21 2016-06-01 北京化工大学 Method for massively preparing platinum-based dealloyed electrocatalyst for cathode of fuel cell
CN107326444A (en) * 2017-07-21 2017-11-07 山东大学 A kind of method that hydro-thermal corrosion porous-substrates grow self-standing gan monocrystalline
CN110158155A (en) * 2019-06-03 2019-08-23 西安奕斯伟硅片技术有限公司 A kind of processing method and processing unit of silico briquette
CN111172597A (en) * 2020-01-21 2020-05-19 河南理工大学 Preparation method of luminescent porous silicon
CN113773517A (en) * 2021-10-08 2021-12-10 上海懿禾嘉朋新材料科技有限公司 General preparation method of multi-stage porous metal organic framework material

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CN105417518A (en) * 2014-09-05 2016-03-23 中国科学院金属研究所 Gas-phase post-treatment modification apparatus and gas-phase post-treatment modification method of solid carbon material
CN105417518B (en) * 2014-09-05 2017-07-07 中国科学院金属研究所 Gas phase post processing reforming apparatus and the method for a kind of solid carbonaceous material
CN105405930A (en) * 2015-12-21 2016-03-16 南昌大学 Micro-droplet etching texturing method for polycrystalline silicon chip for solar battery
CN105405930B (en) * 2015-12-21 2017-04-05 南昌大学 A kind of microlayer model etching etching method of solar cell polysilicon chip
CN105633422A (en) * 2016-03-21 2016-06-01 北京化工大学 Method for massively preparing platinum-based dealloyed electrocatalyst for cathode of fuel cell
CN107326444A (en) * 2017-07-21 2017-11-07 山东大学 A kind of method that hydro-thermal corrosion porous-substrates grow self-standing gan monocrystalline
CN110158155A (en) * 2019-06-03 2019-08-23 西安奕斯伟硅片技术有限公司 A kind of processing method and processing unit of silico briquette
CN111172597A (en) * 2020-01-21 2020-05-19 河南理工大学 Preparation method of luminescent porous silicon
CN111172597B (en) * 2020-01-21 2021-03-26 河南理工大学 Preparation method of luminescent porous silicon
CN113773517A (en) * 2021-10-08 2021-12-10 上海懿禾嘉朋新材料科技有限公司 General preparation method of multi-stage porous metal organic framework material

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